Hydrochloric Acid → 5,5-dimethyl-3-[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]imidazolidine-2,4-dione

HRID 1012959ノート

反応式

HRID 1012959 の反応式
[CH3:1][C:2]([NH:8][C:9](=[O:29])[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH2:17][C:18]2[C:27]3[CH2:26][CH2:25][CH2:24][CH2:23][C:22]=3[C:21](=[O:28])[NH:20][N:19]=2)[CH:12]=1)([CH3:7])[C:3]([O:5]C)=O.[OH-].[Na+].Cl>CN(C=O)C>[CH3:7][C:2]1([CH3:1])[NH:8][C:9](=[O:29])[N:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([CH2:17][C:18]3[C:27]4[CH2:26][CH2:25][CH2:24][CH2:23][C:22]=4[C:21](=[O:28])[NH:20][N:19]=3)[CH:12]=2)[C:3]1=[O:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57786643methyl 2-methyl-2-[[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]carbamoylamino]propanoate

生成物 1

HCID 252212665,5-dimethyl-3-[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]imidazolidine-2,4-dione

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of methyl 2-methyl-2-[[3-[(4-oxo-5,6,7,8-tetrahydro-3H-phthalazin-1-yl)methyl]phenyl]carbamoylamino]propanoate (14) (44 mg, 0.11 mmol) in dry DMF (2 mL) was added finely powdered sodium hydroxide (4 mg, 0.072 mmol). The reaction mixture was immersed in a preheated oil bath at 50° C. for 5 hours, before being neutralized by addition of 1M HCl The desired product was isolated from the resultant solution by preparative chromatography to yield a solid (3.6 mg, 98% purity). M/z (LC-MS, ESP), RT=7.69 mins (M+H 367.1).

出典と根拠

ORDレコード
ord-c485a3fa48f245b0abdaf29b7fbf93f5
出典データセット
uspto-grants-2011_07
特許番号
US07981890B2

反応ノート

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